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lndian Standard
TRISODIUM PHOSPHATE - SPECIFICATION
( Fourth Revision )
UDC 661’833’455’3
0 BIS 1992
_:
General Inorganic Chemicals Sectional Committee, CHD 003
FOREWORD
This Indian Standard ( Fourth Revision ) was adopted by the Bureau of Indian Standards, after the
draft finalized by the General Inorganic Chemicals Sectional Committee had been approved by the
Chemical Division Council.
This standard was originally published in 1954 and then subsequently revised in 1964, 1973 and
1985. In the original standard, three types of trisodium phosphate, namely, anhydrous,
monohydrate and dodecahydrate were covered. These were retained m the first revision. However,
in the second revision, the monohydrate type of trisodium phosphate was deleted as it was not
being manufactured in the country. In the second revision, analytical reagent grade of trisodium
phosphate was added and a new requirement of free sodium hydroxide was incorporated. During
the third revision, a new requirement of free alkalinity was prescribed for dodecahydrate type of
trisodium phosphate, deleting the requirements of carbonates and free sodium hydroxide for this
type. *
In this revision, new requirements of insolubles, soluble silica and chloride contents have been
prescribed for trisodium phosphate, dodecahydrate along with the relevant test methods. Also, the
methods for determination of carbonate alkalinity, phosphate, carbonate, free sodium hydroxide and
total alkalinity have been suitably modified.
NTPC-Ramagundam
of the relative amount of other characteristics.
For the purpose of deciding whether a particular requirement of this standard is complied with, the
final value, observed or calculated, expressing the result of a test or analysis, shall be rounded off in
accordance with IS 2 : 1960 ‘Rules for rounding otf numerical values ( revised )‘. The number of
significant places retained in the rounded off value shall be the same as that of the specified value
in this standard.
IS 573 : 1992
Indian Standard
TRISODIUM PHOSPHATE-SPECIFICATION
(Fourth Revision )
1 SCOPE
4.2 The analytical grade shall be of dodecahydrate
This standard prescribes requirements and methods of type only.
sampling and test for trisodium phosphate.
5 REQUIREMENTS
2 REFERENCES
5.1 Description
The Indian Standards listed below are necessary
adjuncts to this standard: The material shall be in the form of white crystalline
powder or in the form of easily triable small lumps.
IS No. Title
5.2 The material shall comply with the requirements
264 : 1976 Nitric acid ( second revision ) given in Table 1 when tested according to the methods
prescribed in Annex A. Reference to the relevant
265 : 1987 Hydrochloric acid ( third revision )
clauses of Annex A is given in co1 6 of the table.
915 : 1975 One-mark volumetric flask ( first
revision ) 6 PACKING AND MARKING
NTPC-Ramagundam
2263 : 1979 Methods of preparation of indicator 6.2 Marking
solutions for volumetric analysis
(fzrst revision ) The packages shall be legibly marked with the follow-
2316 : 1990 Methods of preparation of ing information:
standard solutions for calorimetric 4 Name, grade and type of the material;
and volumetric analysis ( second
b) Mass of the material;
revision )
4905 : 1968 Methods for random sampling 4 Indication of the source of manufacture;
4 TYPES 7 SAMPLING
4.1 The technical grade material shall be of two types, The method of drawing representative samples of
namely: the material, number of tests to be performed and the
criteria for finding the conformity of the material to
a) Dodecahydrate, and the requirements of this specification shall be as
b) Anhydrous. prescribed in Amrex B.
IS 573 : 1992
NTPC-Ramagundam
vii) Soluble iron compounds 0.009 0.02 0.001 A-S
1 (as Fe), percent by mass, MUX
2
IS 573 : 1992
ANNEX A
(Clause 5.2)
METHODS OF TEST FOR TRISODIUM PHOSPHATE
NTPC-Ramagundam
where
M1 = mass in g of the residue, and
A-3.1.5 Standard Hydrochloric Acid - 0.5 N and
M2 = mass in g of the material taken for test. 0.1 N.
3
*
IS 573 : 1992
removal of the precipitate and place the paper in the A-4.1 Reagents
flask. Dilute to about 100 ml with water. Stopper the
flask and shake it vigorously until the pulp and the A-4.1.1 Barium Chloride Solution - about 10 per-
precipitate are completely disintegrated. Remove the cent.
stopper and wash it with water, returning the wash-
ings to the flask. From a burette add 50 ml of 0.5 N A-4.1.2 Phenolphthalein Indicator Solution - 0.1 g
standard sodium hydroxide solution, shaking the in 100 ml of 60 percent rectified spirit.
flask during addition. Shake vigorously until all the
precipitate dissolves (see Note). Add 1 ml of mixed A-4.13Standard Hydrochloric Acid - 0.1 N.
indicator solution and titrate the excess of sodium
hydroxide solution with 0.5 N hydrochloric acid until A-4.1.4 Methyl Orange Indicator Solution - 0.01 g
the colour changes from violet to green-blue and then in 100 ml of water.
sharply to yellow.
A-4X5 Silver Nitrate Solution - about 5 percent.
NOTE - Examine the disintegrated paper pulp carefully for
specks of undissolved ptwzipitatc which sometimes dissolve in A-4.1.6 Benzyl Alcohol
excess of sodium hydroxide but with difficulty.
A-4.1.7 Methyl Red Indicator Solution - 0.15 g in
A-3.2.1 Carry out a blank determination using all 500 ml of water.
reagents, without the sample and using exactly 0.1 N
A-4.1.8 StanaizrdSodiumHydroxideSolutio -0.1 N.
standard sodium hydroxide solution and 0.1 N
standard hydrochloric acid instead of 0.5 N acid and A-4.2 Procedure
0.5 N alkali.
A-4.2.1 Weigh accurately about 5 g of the material in
case of dodecahydrate grade and 2.5 g of the material
A-3.3 Calculation in case of anhydrous grade and dissolve it in water.
Filter off insolubles, if any, and make up the filtrate
Phosphates (as Pro,), percent by mass = and the washings to 250 ml in a volumetric flask.
NTPC-Ramagundam
and the carbonates are precipitated off. Add 0.2 ml of
where phenolphthalein indicator and titrate with standard
hydrochloric acid to colourless end point (VI).
v, = volume in ml of 0.5 N sodium hydroxide
solution used with the sample, A-4.2.3 Transfer 25 ml aliquot of the solution pre-
pared in A-4.2.1 to a 250~ml beaker, add 1 drop of
v, = volume in ml of 0.5 N hydrochloric acid
methyl orange indicator and titrate with standard hydm-
used with the sample,
chloric acid to light pink end point (V,).
v3 = volume inml ofO.1 Nsodium hydroxide
used in the blank, A-4.2A Add sufficient silver nitrate solution to pre-
cipitate all the phosphate (35 to 40 ml are usually
v, = volume in ml of 0.1 N hydrochloric acid sufficient), 2 ml of benzyl alcohol to coagulate all the
used in the blank, and precipitate and 0.5 ml of methyl red indicator. Titrate
M = mass in gof the material contained in the the liberated nitric acid with standard sodium hy-
solution, taken for the precipitation. droxide solution. The end point shall be from red to
yellow (V,).
A-4 DETERMINATION OF CARRONATE A-4.3 Calculation
ALKALINITY AND PHOSPHATE,
CARBONATE, FREE SODIUM Phosphate (as Pro&, percent by mass
HYDROXIDE AND TOTAL ALKALINITY
v. x 3.55
3
iu
In analiquot of the solution of the material, total alkali Free sodium hydroxide (as NaOH), percent by
and phosphates are titrated with a standard acid. The mass
acid phosphates formed is precipitated with silver v, x 4.0
nitrate and the free acid liberated is titrated with alkali =
which gives the phosphate content. In another aliquot iu
of the solution, carbonates and phosphates are precipi-
Carbonates (as Na,CO& percent by mass
tated with barium chloride and free alkali is deter-
mined by titration with standard hydrochloric acid.
(V, - vr - V,) x 530
Carbrnate alkalinity is then determined from the data =:
obtamed. M
4
IS 573 : 1992
Total alkalinity (as NaOI-I), percent by mass blank at 535mn using green filter No. 4 and 4-cm cell
(use l-cm cell if the colour is too strong). Draw a cali-
(V, - V,) x 4.0 bration curve by plotting concentration (in clg/ml)
= against absorbance.
iu
Carbonate alkalinity (as NaOH), percent by mass A-5.3.1 Weigh accurately about 1 g of the material
and dissolve in 20 ml of water. Add 5 ml of dilute
= (V, - v, - V,) x 4.0 hydrochloric acid, stir slowly with a glass rod, cover
with watch glass and boil gently for 15 to 20 minutes.
M Cool and transfer to a one-mark graduated flask.
Add 4 ml of sodium citrate solution or 2 ml of ammo-
where nium citrate solution, 5 ml of thioglycollate reagent
iu = mass in g of the material taken for the and 15 ml of ammonium hydroxide. Dilute to the
test. mark and after 10 minutes determine the absorbance at
535~run using green filter No. 4 and 4-cm cell (use
l-cmcell if the colour is too strong). Read the concen-
A-5 DETERMINATION OF SOLUBLE IRON
COMPOUNDS trations (in ml) of this solution from the calibration
curve and ca V culate total amount of soluble iron ores-
ent (as Fe).
A-5.0 Outline of the Method
Iron is determined calorimetrically by measuring the A-6 DETERMINATION OF NITROGEN
transmittance of reddish-violet colour produced by COMPOUNDS
ferrous and ferric iron with thioglycollic acid atpH 10.
A-6.1 Apparatus
A-5.1 Apparatus
A-6.1.1 Nesskr Cylinders - 50 ml capacity.
A-5.1.1 Photoelectric Absorptiometer
A-6.2 Reagents
NTPC-Ramagundam
A-S.2 Reagents
A-6.2.2 Devarda ‘s Alloy - consisting of copper 50
A-5.2.1 Dilute Hydrochloric Acid - approximately parts, aluminium 45 parts and zinc 5 parts.
5 N.
A-6.2.3 Nessler Solution
A-5.2.2 Sod&r Citrate Solution (1 M) or Ammonium
Citrate Solution (2 M) - 29.4 g of sodium citrate in Dissolve 10 g of potassium iodide in 10 ml of ammo-
100 ml of water or 43.0 gof ammonium citrate nia-free water, and add to it slowly with stirring satu-
in 100 ml of water. rated mercuric chloride solution until a slight perma-
nent precipitate forms. Add 30 g of potassium hydrox-
A-5.23 Ammonium Hydroxide - approximately 16 ide and when it has dissolved, add 1 ml more ‘of
N. mercuric chloride solution, and dilute to 200 ml with
ammonia-free water. Allow to settle overnight, decant
A-5.2.4 Thioglycollate Reagent the clear solution and keep it in a bottle closed with a
Add 20 ml of ammonium hydroxide in 30 ml of water, well-fitting rubber stopper.
then add a mixture comprising 10 ml of thioglycollic
acid and 40 ml of water. A-6.2A Dilute Hydrochloric Acid - same as
in A-5.2.1.
A-5.2.5 Standard Iron Solution
A-6.2.5 StandardAmmonium Chloride Solution
Dissolve 0.702 g of ferrous ammonium sulphate in
10 ml of dilute sulphuric acid [lo percent (v/v)] and Dissolve 0.382 g of ammonium chloride in water and
dilute with water to 1 000 ml. Take 10 ml of this make up to exactly 100 ml. Take 10 ml of the solution
solution and dilute to 100 ml. One millilitre of this and dilute to exactly 1 000 ml. One millilitre of this
solution contains 0.01 mg of iron (as Fe). solution contains 0.01 mg of nitrogen (as N).
Take several aliquots of the standard iron solution in Weigh 1.0 g of the material and dissolve in 50 ml of
one-mark graduated flasks, add to each of these flasks water. Add 20 ml of sodium hydroxide solution, 0.5 g
4 ml of sodium citrate solution or 2 ml of ammonium of powdered Devarda’s alloy and allow to stand for 2
citrate solution, 5 ml of thioglycollate reagent and hours in a distillation flask protected from loss or gain
15 ml of ammonium hydroxide, swirling after each of ammonia. Then slowly distil30 to 35 ml into 5 ml
addition. Dilute to the mark and mix well. After 10 of water containing 1 drop of dilute hydrochloric acid.
minutes, determine the absorbance against a reagent Transfer to a Nessler cylinder, add 1 ml of sodium acid.
5
IS 573 : 1992
Transfer to a Nessler cylinder, add 1 ml of sodium A-9.2 Reagents
hydroxide solution and 2 ml of Nessler solution. Make
up the volume to SO-ml mark. Carry out a control test A-9.2.1 Acetic Acid - approximately 33 percent.
in another Nessler cylinder using for compar ison 1 ml
of standard ammonium chloride solution in place of A-9.2.2 Dilute Ammonium Hydroxide - approxi-
the material and the same quantities of other reagents mately 10 percent.
in the same total volume of the reaction mixture.
A-9.2.3 Hydrogen Peroxide - approximately 6 per-
A-6.3.1 The limit prescribed in Table 1 shall be con- cent.
sidered as not having been exceeded if the intensity
of the colour produced in the test with the material is A-9.2A Potassium Cyanide Solution
not greater than that produced in the control test.
Dissolve 10 g of potassium cyanide in 90 ml of water,
A-7 DETERMINATION OF SULPHATES add 2 ml of hydrogen peroxide, allow to stand for 24
hours and make up to 100 ml with water.
A-7.1 Reagents
A-9.2.5 Concentrated Nitric Acid - See IS 264 :
A-7.1.1 Dilute Hydrochloric Acid - same as 1976.
in A-5.2.1.
A-9.2.6 Standard Lead Solution
A-7.1.2 Barium Chloride Solution - same as
Dissolve 1.60 gof lead nitrate [Pb(NO,) ] in water and
in A-4.1.1.
make up the solution to 1000 ml exactly .%pette out 10
ml of the solutionand dilute again ina volumetric flask
A-7.2 Procedure
to 100 ml with water. One millilitre of this solution
Weigh accurately about 10 g of the material and dis- contains 0.1 mg of lead (as Pb).
solve in 100 ml of water and 2 ml of dilute hydrochlo-
ric acid.. Filter, if necessary; heat the filtrate to boil- A-9.2.7 Sodium Sulphi& Solution - approximately
ing; add slowly, with constant stirring, 5 ml of barium 10 percent.
NTPC-Ramagundam
and dissolve in 30 ml of hot water. Add 5 ml of acetic
acid. Make it alkaline to litmus by gradual addition of
A-7.3 Calculation
dilute ammonium hydroxide and add 1 ml of potas-
Sulphates (as SO,), percent by mass sium cyanide solution. Carry out a control test in
another Nessler cylinder using 2.0 g of the material,
0.5 ml of standard lead solution and the same quantities
= 41.15 2 of other reagents. Filter both the solutions, if they
2 are turbid, and if the colours of the solutions differ,
where equalize by the addition of a few drops of a highly
diluted solution of burnt sugar or other non-reactive
it4, = mass in g of the precipitate, and substance. Dilute both the solutions with water and
M, = mass in g of the material taken for the make up the volume of each to 50 ml. Add 2 drops of
test. sodium sulphide solution, mix thoroughly and com-
pare the colours developed in the two cylinders after
A-8 DETERMINATION OF ARSENIC 5 minutes.
6
IS 573 : 1992
A-10.1.4 Oxalic Acid - 10 percent (m/v). A-11.2.2 Silver Nitrate - 10 percent solution in
NTPC-Ramagundam
A-10.1.5 Standard Silica Solution
at 140%) in chloride free water and dilute to 1000 ml.
Fuse 1 g of high purity quartz with 4 g of sodium One millilitre of this solution contains 500 mg of
carbonate (AR Grade) in a platinum crucible at chloride as Cl.
1 oooOC. Dissolve the residue in silica free water and
dilute to 1000 ml in a volumetric flask. One ml of this A-113 Procedure
solution is equivalent to 1 mg of silica (as SiOJ. Store
the solution in polyethylene bottles. Dissolve 1 g of the sample in 20 ml of water and add
3 ml of concentrated nitric acid and 1 ml of 10 percent
A-10.2 Procedure silver nitrate solution. Dilute to 50 ml in a Nessler
cylinder. The turbidity produced shall not be greater
Dissolve 5 g of the sample in 250 ml of water. Dilute than that produced by 2 ml of standard chloride solu-
10 ml of this solution to 250 ml. Pipette 50 ml of the tion for technical grade and 1 ml of AR Grade of
clear sample solution into a polyethylene container. material diluted to the same volume with all the
Add 1 ml of 1: 1 hydrochloric acid solution. Add 4 ml reagents.
7
IS 573 : 1992
ANNEX B
(Clause 7)
B-l GENEBAL REQUIREMJZNTS OF SAMPLING Arrange all the containers in the lot in a systematic
manner and starting from any container count them as
B-1.0 In drawing, preparing, storing and handling 1,2,3, .... up to r, where r is the integral part of N/n (N
samples, the followingprecautions and directions shall and n being the lot size and sample size respectively).
be observed. Every rth container thus counted shall be drawn to
constitute the sample.
El.1 Samples shall not be takenat a place exposed to
the adverse effects of weather. Table 2 Number of Containers to be Selected
from Lots of Different Sizes
B-l.2 The sampling instruments and sample contain- (Chuse B-2.2)
ers shall be clean and dry. JAtSizc SampleSize
B-l.5 The samples shall be placed in suitable, clean, 801 and above 10
NTPC-Ramagundam
to B-2.3 draw with anappropriate sampling instrument
that they are almost completely filled by the sample.
a representative portion of the material, sufficient for
carrying out the tests specified under 5. These shall
B-l.7 Each sample container shall be suitably stop-
constitute the individual samples.
pered and sealed air-tight after filling, and marked
with full particulars of the material (see 6.2), the date B-3.2 From each of the individual samples, a small
of sampling and the lot and batch number. but equal quantity of the material shall be taken and
thoroughly mixed to constitute a composite sample.
B-l.8 Samples shall be stored in a cool and dry place.
B-3.3 The material in the individual and composite
B-2 SCALE OF SAMPLING test samples shall be divided into three equal parts and
transferred to separate bottles, sealed and labelled
B-2.1 Lot with full identification particulars of the samples
All the containers in a single consignment of the (see B-1.7). The material in each such bottle shall
material drawn from a single batch of manufacture constitute a test sample. Separate these test samples
shall constitute a lot. If a consignment is declared or representing individual and the composite samples
known to consist of different batches of manufacture, into three identical sets of test samples.
the batches shall be marked separately and the group of
containers in each batch shall constitute separate lots. B-3.4 Distribution of Test Samples
One set of test samples shall be sent to the purchaser
B-2.1.1 Samples shall be tested for each lot for ascer- and another to the supplier. The third set of test
taining the conformity of the material to the require- samples bearing the seals of the purchaser and the
ments of the specification. supplier shall constitute the referee sample to be used
in case of dispute between the purchaser and the
B-2.2 The number(n) of containers to be selected at supplier, and shall be kept at a place agreed to between
random from the lot shall depend on the size of the lot the purchaser and the supplier.
and shall be in accordance with Table 2.
8
IS 573 : 1992
B-4.2 Tests for determination of the remaining char- B-5.1.1 For declaring the conformity of the lot to the
acteristicsshallbeperformedonthecompositesample. sp@kd requirement of matter insoluble in water,
(X + 0.6 R) computed from test results shall be less
B-5 CRITERIA FOR CONFORMITY than or equal to the relevant limits prescribed in
Table 1. The conformity criterion for phosphate shall
B-5.1 For individual samples for those characteristics be that (X - 0.4 R) computed from test results shall be
which are tested on individual samples, the mean and greater than or equal to the relevant limits prescribed
range of test results shall be computed as follows: in Table 1.
I I
I Standard Mark
The use of the Standard Mark is governed by the provrstons of the Bureau of Indian
I
Stundurds Act, 1986 and the Rules and Regulations made thereunder. The Standard Mark on
products covered by an Indian Standard conveys the assurance that they have been produced
to comply with the requirements of that standard under a well defined system of inspection,
testing and quality control which is devised and supervised by BlS and operated by the
producer. Standard marked products are also continuously checked by BIS for conformity
to that standard as a further safeguard. Details of conditions under which a licence for the
use of the Standard Mark may be granted to manufacturers or producers may be obtained
from the Bureau of Indian Standards.
1 1
Bureau of Indian Standards
BIS is a statutory institution established under the Bureau of Indian Srandurds Act, 1986 to promote
harmonious development .of the activities of standardization. marking and quality certification of goods
and attending to connected matters in the country.
Copyright
BIS has the copyright of all its publications. No part of these publications may be reproduced In
any form without the prior permission in writing of UIS. This does not preclude the free use, in the
course of implementing the standard, of necessary details, such as symbols and sizes, type or grade
designations. Enquiries relating to copyright be addressed to the Director ( Publications ), BIS.
Indian Standards are reviewed periodically and revised, when necessary and amendments, if any, are
issued from time to time. Users of Indian Standards should ascertain that they are in possession of
the latest amendments or edition. Comments on this Indian Standard may be sent to BIS giving the
following reference :
Headquarters:
_ _ r
AMENDiVENT NO. 1 JULY 1993
TO
NTPC-Ramagundam
(Page 2, Table 1 ) -Add the following note at the end of Table 1:
‘NOTE - ?he requiremcots for soluble silica ( as Sio;! ) and chloride ( as Cl ) for rri~..dium
phosphate, tinicA, dodecahydrate grade shall be special requirements only for the material
intended IO be used for softening water and for prevention of hard boiler scale.’
(CHDOO3)